The preparation of four cereal reference materials (two wheat and two maize) and the certification of their 4‐deoxynivalenol (DON) contents is described. The materials were prepared and certified within the BCR programme of the Commission of the European Community as part of a broad activity to improve accuracy and agreement of measurements of importance in food and agriculture. Reference material RM 379 was prepared from naturally contaminated wheat four blended with ‘blank’ material to achieve the desired DON content. The reference material RM 378 was prepared from naturally contaminated maize identified as containing approximately the desired DON content. Details are given of the milling, blending and packaging procedure, and the checks to ensure homogeneity and stability of the materials. The reference materials RM 396 and 377 were similarly prepared from the blank wheat and maize samples respectively. The certification exercise was carried out by five laboratories (with a further two to three laboratories providing supporting data) using a variety of extraction and clean‐up procedures with either high performance liquid chromatography (HPLC) or gas chromatography (GC) as the determinative stages.